[Development of a portable micro-liquid chromatograph]

Abstract

Portable analytical instruments find extensive application in on-site examination because of their significant advantages: these instruments are convenient and easy-to-carry, leading to high time-effectiveness, and involve low reagent consumption. We report a portable micro-liquid chromatograph (p-μLC) that was designed and fabricated in our laboratory. The p-μLC integrates homemade dual large-thrust syringe pumps for delivering the mobile phase, a capillary polymer monolithic column as the stationary phase for the separation of the target analytes, and a specially designed dual-functional optical-fiber microflow-cell for online detection. The dual-thrust syringe pumps can realize isocratic and/or gradient elution as well as reloading of the mobile phase, with flow rates ranging from 0.025 μL/min to 5.6 mL/min and the maximum working pressure of 4.5 MPa. The polymethacrylate based C-18 monolithic column facilitates the separation of small organic molecules and biomacromolecules. A homemade high-power light emission diode (LED) light source and a modified xenon flash lamp are assembled as the light source module. The dual-functional detector consists of an optical fiber microflow-cell with a self-focusing lens and a light-guiding capillary, light source module, and a small-sized grating spectrometer with an output wavelength range of 400-680 nm for the LED light source and 220-700 nm for the xenon flash lamp, enabling online detection of the absorption and fluorescence spectra of the analytes from 220 to 700 nm. A bifurcated optical fiber bundle is prepared and used to connect the light source, microflow-cell, and grating spectrometer so that the incident light leading-in and the fluorescence/scatting light leading-out can be realized simultaneously. The junction end of the bifurcated optical fiber bundles connects to one end of the light path of the microflow-cell, and a straight-through optical fiber connects another end of the microflow-cell. In the UV-Vis absorption mode, the straight-through optical fiber reads out the transmitted light, while in the fluorescence mode, the excitation light beam from the light source irradiates the sample solution in the flow-cell via one branch of the bifurcated optic fiber bundles. The fluorescence leading-out via the other branch of the bifurcated optical fiber bundles in the opposite direction of the excitation light beam is read out by the spectrometer. All the large-thrust syringe pumps and flow-path, capillary monolithic column, and optical fiber mediated flow-cell detection as well as controlling modules are installed in a suitcase with a total weight of less than 8 kg. The p-μLC is powered by DC 12V 3A or 18650 lithium battery pack and controlled by a panel computer with a custom-built windows-based chromatography workstation software for data acquisition. When using the home-made polymethacrylate based C-18 monolithic capillary column (530 μm ID×200 mm in length), the mixed alkylbenzenes can be separated and detected in an isocratic elution mode. The separation efficiency is comparable to that obtained with a commercially available HPLC.

Keywords: capillary monolithic column; dual-functional ultraviolet-visible/fluorescence micro-detector; large-thrust syringe pump; portable micro-liquid chromatograph (p-μLC).